CN1405800A - High magnetoconductivity low-temperature sintered medium-high frequency stacked chip inductive material and its preparation method - Google Patents
High magnetoconductivity low-temperature sintered medium-high frequency stacked chip inductive material and its preparation method Download PDFInfo
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- CN1405800A CN1405800A CN 02146687 CN02146687A CN1405800A CN 1405800 A CN1405800 A CN 1405800A CN 02146687 CN02146687 CN 02146687 CN 02146687 A CN02146687 A CN 02146687A CN 1405800 A CN1405800 A CN 1405800A
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- 239000000463 material Substances 0.000 title claims abstract description 45
- 230000001939 inductive effect Effects 0.000 title claims description 16
- 238000002360 preparation method Methods 0.000 title claims description 9
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims description 52
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 42
- 239000011701 zinc Substances 0.000 claims description 24
- 238000009766 low-temperature sintering Methods 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000004615 ingredient Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 238000000465 moulding Methods 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 5
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 229910001308 Zinc ferrite Inorganic materials 0.000 claims description 3
- KOMIMHZRQFFCOR-UHFFFAOYSA-N [Ni].[Cu].[Zn] Chemical group [Ni].[Cu].[Zn] KOMIMHZRQFFCOR-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000008139 complexing agent Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000035699 permeability Effects 0.000 abstract description 16
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 abstract 1
- 230000005415 magnetization Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910000608 Fe(NO3)3.9H2O Inorganic materials 0.000 description 2
- 241000409201 Luina Species 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- DSUJCACXEBHAAS-UHFFFAOYSA-N 3,7,8,10-tetramethylbenzo[g]pteridine-2,4-dione Chemical compound CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)N(C)C2=O DSUJCACXEBHAAS-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- Magnetic Ceramics (AREA)
Abstract
The invention discloses the technique area of preparing the material of the inductor. Ag is as the internal electrode. The electrode, the soft magnetization ferrite and the burning rate accelerator are sintered at 860-950 deg.C so as to obtain the sheet shaped medium high frequency MLCI inductance material with high magnetic permeability. The room temperature initial permeability of the material can be controlled in 600-1000. The size of the ceramics crystal grain is less than 2 microns. Comparing with the prior art, the invention makes the permeability of the material raise to 1000. The method is suitable to the production of the sheet shaped inductance element with large capacity and small size. The invention provides the features of simple formula and technique, stable performance.
Description
Technical field
The invention belongs to inductive material technology of preparing scope, particularly high magnetoconductivity low temperature sintering medium-high frequency multilayer chip inductor material and preparation method thereof.
Background technology
The process technology key of preparation laminated chip inductor (Multi-layer Chip Inductors or Multi-layer Ferrite Inductor is called for short MLCI or MLFI) is that magnetic media material and internal conductor material (being generally the Ag electrode) are burnt altogether.This has lower sintering temperature with regard to requiring soft magnetic ferrite wherein, has high magnetic permeability and high quality factor simultaneously.The material of general sense of medium-high frequency both at home and abroad mainly is the NiCuZn soft magnetic ferrites at present.Add CuO formation NiCuZn ferrite solid solution for reducing sintering temperature, sintering temperature can be reduced to 1050 ℃, and then adds sintering agent, and sintering temperature is reduced to below 900 ℃.But because the adding of sintering agent descends magnetic property, initial permeability reduces.General used sense material initial permeability is the highest about 400.Adopt the NiCuZn ferrite nano powder magnetic permeability of chemical method preparation to reach about 600, but in sintering process, occur the inhomogeneous of crystal grain easily and grow up unusually, the repeatability of material property is had certain influence.Therefore preparation and sintering process how to control NiCuZn ferrite nano powder are problems to be solved by this invention with the MLCI material that obtains thin crystalline substance, high magnetic permeability and stable performance.
Summary of the invention:
The purpose of this invention is to provide a kind of high magnetoconductivity low temperature sintering medium-high frequency laminated inductive material and preparation method thereof.Described laminated inductive material is made up of major ingredient and auxiliary material, it is characterized in that: described major ingredient is a nickel-copper-zinc ferrite, and its molecular formula is (Ni
0.2-xCu
0.2Zn
0.6+xO) (Fe
2-yMn
yO
3+0.5y)
1-z, 0≤x≤0.1,0≤y≤0.05,0≤z≤0.10 wherein; Described auxiliary material is low-temperature sintering sintering agent bismuth oxide Bi (NO
3)
3Described major ingredient shared mass percent in prescription is 99~100%, and described auxiliary material sintering agent content is 0~1.0%.
The initial feed of described major ingredient is Fe (NO
3)
3, Ni (CH
3COO)
2, Cu (CH
3COO)
2, Zn (CH
3COO)
2, Mn (CH
3COO)
2Or nitrate and the citric acid of Ni, Cu, Zn, Mn.
Concrete processing step is as follows:
1. with initial feed Fe
3+With citric acid according to stoichiometric proportion wiring solution-forming, wherein Fe
3+The concentration of ion between 0.5~5M, Fe
3+And the citric acid mol ratio is between 0.5~1.5;
2. with Ni
2+, Zn
2+, Cu
2+, Mn
2+, Bi
3+Salt add in the solution 1. be made into according to stoichiometric proportion, and add mass ratio be 5~10% PEG as complexing agent, be heated to 80~100 ℃ of reactions two hours, form stable sols;
3. the colloidal sol that 2. step is generated places 120~150 ℃ baking oven to dry, and forms xerogel;
4. xerogel in 600~800 ℃ of pre-burnings, is incubated 2~6 hours in high temperature furnace, can obtain the ambrose alloy Zn soft magnetic ferrite powder of nanoscale thickness;
5. with above-mentioned powder through ball milling 6~8 hours, be that medium gets ultra-fine ambrose alloy Zn soft magnetic ferrite slurry with water or ethanol;
6. the oven dry of the slurry behind the ball milling is crossed 100~200 mesh sieves, granulation, moulding;
7. green sintering can adopt normal sintering and two-part sintering process.(a) normal sintering is about to the molding mass that 6. step generate and is warming up to 860~950 ℃ of insulations 120~360 minutes in high temperature furnace.(b) two-part sintering is about to the molding mass that 6. step generate and is warming up to 910~950 ℃ in high temperature furnace, and of short duration insulation 0~10 minute was cooled to 860~900 ℃ of sintering 120~360 minutes then, can obtain high magnetoconductivity low temperature sintered chip inductive material.
The invention has the beneficial effects as follows that the low-temperature sintering prescription is adjustable, technology is simple and easy to do, favorable repeatability, firing temperature is low, burn till wide temperature region (860~950 ℃), the low temperature sintered ferrite material stable performance that obtains, good reliability has high initial permeability 600~1000 and high specific insulation 10
10Ω cm.Compared with prior art, has the magnetic permeability height, low cost of manufacture, the characteristics of process stabilizing, be easy to suitability for industrialized production, be a kind of high performance sheet sense material of new generation, satisfy the requirement of high reliability medium-high frequency lamination sheet sense material fully, provide possibility for further dwindling component size and improving inductance value.It can make the magnetic permeability of low sintering inductive material improve.
Description of drawings
Fig. 1 (a) and (b) are sintering curres of embodiment 1 sample, and wherein Fig. 1 (a) curve 1 is the two-part sintering, and curve chart 1 (b) is a normal sintering.
Fig. 2 is the magnetic spectral characteristic curve of embodiment 1 sample.
Fig. 3 is the quality factor curve of embodiment 1 sample.
Fig. 4 is the magnetic spectral characteristic curve of embodiment 2 samples.
Fig. 5 is the quality factor curve of embodiment 2 samples.
Embodiment
The present invention is high magnetoconductivity low temperature sintering medium-high frequency laminated inductive material and preparation method thereof.Described laminated inductive material is made up of major ingredient and auxiliary material, and the initial feed of described major ingredient is Fe (NO
3)
3, Ni (CH
3COO)
2, Cu (CH
3COO)
2, Zn (CH
3COO)
2, Mn (CH
3COO)
2Or the molecular formula of the nickel-copper-zinc ferrite of the nitrate of Ni, Cu, Zn, Mn and citric acid is: (Ni
0.2-xCu
0.2Zn
0.6+xO) (Fe
2-yMn
yO
3+0.5y)
1-z, 0≤x≤0.1,0≤y≤0.05,0≤z≤0.10 wherein; Described auxiliary material is low-temperature sintering sintering agent bismuth oxide Bi (NO
3)
3Described major ingredient shared mass percent in prescription is 99~100%, and described auxiliary material sintering agent content is 0~1.0%.
Described major ingredient initial feed is Fe (NO
3)
3, Ni (CH
3COO)
2, Cu (CH
3COO)
2, Mn (CH
3COO)
2Or nitrate and the citric acid of Ni, Cu, Zn, Mn.
Concrete processing step is as follows:
1. with initial feed Fe
3+With citric acid according to stoichiometric proportion wiring solution-forming, wherein Fe
3+The concentration of ion between 0.5~5M, Fe
3+And the citric acid mol ratio is between 0.5~1.5;
2. with Ni
2+, Zn
2+, Cu
2+, Mn
2+, Bi
3+Salt add in the solution 1. be made into according to stoichiometric proportion, and add mass ratio be 5~10% PEG as complexing agent, be heated to 80~100 ℃ of reactions two hours, form stable sols;
3. the colloidal sol that 2. step is generated places 120~150 ℃ baking oven to dry, and forms xerogel;
4. xerogel in 600~800 ℃ of pre-burnings, is incubated 2~6 hours in high temperature furnace, can obtain ultra-fine (nanometer) ambrose alloy Zn soft magnetic ferrite powder;
5. with above-mentioned powder through ball milling 6~8 hours, be that medium gets ultra-fine ambrose alloy Zn soft magnetic ferrite slurry with water or ethanol;
6. the oven dry of the slurry behind the ball milling is crossed 100~200 mesh sieves, granulation, moulding;
7. green sintering can adopt normal sintering and two-part sintering process.(a) normal sintering is about to the molding mass that 6. step generate and is warming up to 860~950 ℃ of insulations 120~360 minutes in high temperature furnace.(b) two-part sintering is about to the molding mass that 6. step generate and is warming up to 910~950 ℃ in high temperature furnace, and of short duration insulation 0~10 minute was cooled to 860~900 ℃ of sintering 120~360 minutes then, can obtain high magnetoconductivity low temperature sintered chip inductive material.For example the present invention is illustrated again below:
Embodiment 1, and chemical method synthesizes NiZnCu soft magnetic ferrite superfine powder, and bismuth oxide is a sintering agent.Initial feed is Fe (NO
3)
3, Ni (CH
3COO)
2, Cu (CH
3COO)
2, Zn (CH
3COO)
2, Mn (CH
3COO)
2, soluble-salt and citric acid.Composition is (Ni
0.15Cu
0.2Zn
0.65O) (Fe
1.98Mn
0.02O
3.01)
0.992, sintering agent Bi (NO
3)
3Be 0.1~0.5wt%.With initial feed Fe (NO
3)
3.9H
2O and citric acid are according to the stoichiometric proportion wiring solution-forming, then by filling a prescription stoichiometry Ni (CH
3COO)
2, Cu (CH
3COO)
2, Zn (CH
3COO)
2, Mn (CH
3COO)
2Add above-mentioned solution, stir, obtain dark-brown colloidal solution.The colloidal solution drying, calcining obtains rufous NiCuZn ferrite superfine powder.Powder carries out ball milling with zirconia ball, after the drying, sieves granulation, moulding, sintering.Fig. 1 (a) and (b) are the sintering curre of embodiment 1 sample, and wherein curve 1 is the two-part sintering among Fig. 1 (a), and curve 2 is a normal sintering among Fig. 1 (b).Carry out the sample that sintering obtains according to curve among Fig. 11 and curve 2 respectively and be designated as sample 1-1 and 1-2.The annulus sample, external diameter 20mm, internal diameter 10mm, thickness 3mm, briquetting pressure 8MPa; Wafer sample, diameter 10mm, thickness 1mm, briquetting pressure is 2MPa.The disk that burns till is measured its resistivity by the silver back up and down.(1K~40MHz) electric impedance analyzer is measured the magnetic frequency spectrum to the annulus sample that burns till, and (5Hz~13MHz) the low-frequency impedance analyzer is measured magnetic temperature spectrum with HP4192A with HP4194A.Fig. 2 provides the magnetic spectral characteristic curve of sample, and two-part sintering initial permeability is about 970, and quality factor are seen shown in Figure 3.The properties of sample parameter that obtains sees Table 1.
Table 1
Sample number into spectrum | Initial permeability | Resistivity (Ω cm) | Than temperature coefficient (/ ℃) | Quality factor |
????1-1 | ????970 | ????4.73×10 10 | ????3.21×10 -6 | ?????28 |
????1-2 | ????780 | ????5.19×10 10 | ????8.12×10 -6 | ?????24 |
Embodiment 2, and chemical method synthesizes NiZnCu soft magnetic ferrite superfine powder, and bismuth oxide is a sintering agent.Initial feed is Fe (NO
3)
3, Ni (CH
3COO)
2, Cu (CH
3COO)
2, Zn (CH
3COO)
2, Mn (CH
3COO)
2, soluble-salt and citric acid.Composition is (Ni
0.15Cu
0.2Zn
0.65O) (Fe
1.99Mn
0.01O
3.01)
0.99, sintering agent Bi (NO
3)
3Be 0.1~0.5wt%.With initial feed Fe (NO
3)
3.9H
2O and citric acid are according to the stoichiometric proportion wiring solution-forming, then by filling a prescription stoichiometry Ni (CH
3COO)
2, Cu (CH
3COO)
2, Zn (CH
3COO)
2, Mn (CH
3COO)
2Add above-mentioned solution, stir, obtain dark-brown colloidal solution.The colloidal solution drying, calcining obtains rufous NiCuZn ferrite superfine powder.Powder steel ball ball milling after the drying, sieves, granulation, and moulding is done parallel laboratory test according to 1 sintering of curve among Fig. 1 respectively, is designated as sample 2-1,2-2, and 2-3.The annulus sample, external diameter 20mm, internal diameter 10mm, thickness 3mm, briquetting pressure 8MPa; Wafer sample, diameter 10mm, thickness 1mm, briquetting pressure is 2MPa.The disk that burns till is measured its resistivity by the silver back up and down.(1K~40MHz) electric impedance analyzer is measured the magnetic frequency spectrum to the annulus sample that burns till, and (5Hz~13MHz) the low-frequency impedance analyzer is measured magnetic temperature spectrum with HP4192A with HP4194A.Fig. 4 provides the magnetic spectral characteristic curve of sample, and two-part sintering initial permeability all about 850, see shown in Figure 5 by quality factor.The properties of sample parameter that obtains sees Table 2.
Table 2
Sample number into spectrum | Initial permeability | Resistivity (Ω cm) | Than temperature coefficient (/ ℃) | Quality factor |
????2-1 | ????840 | ????7.05×10 9 | ????2.14×10 -6 | ????34 |
????2-2 | ????820 | ????6.43×10 9 | ????2.21×10 -6 | ????32 |
????2-3 | ????825 | ????6.91×10 9 | ????2.17×10 -6 | ????32 |
Above-mentioned example explanation, the adjustment by prescription and technology in 860~950 ℃ temperature range, has prepared the medium-high frequency inductive material of low-temperature sintering high performance.Add a small amount of sintering agent, realized low-temperature sintering, the sintering character of material is good, density is high, and by new sintering process---two-part sintering, has improved the microstructure of material, has improved magnetic property.Low-temperature sintering, material room temperature magnetic permeability can be controlled at 600~1000, and cut-off frequency is at 4~14MHz, and resistivity is greater than 10
9Ω cm is not more than 10 than rate of temperature change
-5/ ℃.The uniform crystal particles of material, crystallite dimension≤2 μ m can be used for big sensibility reciprocal chip inductor, is a kind of MLCI material with wide application prospect.And experiment shows the stable performance and the reproducibility excellence of material of the present invention.
Claims (3)
1. high magnetoconductivity low temperature sintering medium-high frequency laminated inductive material, described laminated inductive material is made up of major ingredient and auxiliary material, it is characterized in that: described major ingredient is a nickel-copper-zinc ferrite, its molecular formula is (Ni
0.2-xCu
0.2Zn
0.6+xO) (Fe
2-yMn
yO
3+0.5y)
1-z, 0≤x≤0.1,0≤y≤0.05,0≤z≤0.10 wherein; Described auxiliary material is low-temperature sintering sintering agent bismuth oxide Bi (NO
3)
3Described major ingredient shared mass percent in prescription is 99~100%, and described auxiliary material sintering agent content is 0~1.0%.
2. according to the described high magnetoconductivity low temperature sintering of claim 1 medium-high frequency laminated inductive material, it is characterized in that: the initial feed of described major ingredient is Fe (NO
3)
3, Ni (CH
3COO)
2, Cu (CH
3COO)
2, Zn (CH
3COO)
2, Mn (CH
3COO)
2Or nitrate and the citric acid of Ni, Cu, Zn, Mn.
3. the preparation method of the described high magnetoconductivity low temperature sintering of claim 1 medium-high frequency laminated inductive material is characterized in that:
1. with initial feed Fe
3+With citric acid according to stoichiometric proportion wiring solution-forming, wherein Fe
3+The concentration of ion between 0.5~5M, Fe
3+And the citric acid mol ratio is between 0.5~1.5;
2. with Ni
2+, Zn
2+, Cu
2+, Mn
2+, Bi
3+Salt add in the solution 1. be made into according to stoichiometric proportion, and add mass ratio be 5~10% PEG as complexing agent, be heated to 80~100 ℃ of reactions two hours, form stable sols;
3. the colloidal sol that 2. step is generated places 120~150 ℃ baking oven to dry, and forms xerogel;
4. xerogel in 600~800 ℃ of pre-burnings, is incubated 2~6 hours in high temperature furnace, can obtain the ambrose alloy Zn soft magnetic ferrite powder of nanoscale thickness;
5. be medium ball milling 6~8 hours with above-mentioned powder warp with water or ethanol, get ultra-fine slurry;
6. the oven dry of the slurry behind the ball milling is crossed 100~200 mesh sieves, granulation, moulding;
7. green sintering can adopt normal sintering and two-part sintering process.(a) normal sintering is about to the molding mass that 6. step generate and is warming up to 860~950 ℃ of insulations 120~360 minutes in high temperature furnace.(b) two-part sintering is about to the molding mass that 6. step generate and is warming up to 910~950 ℃ in high temperature furnace, and of short duration insulation 0~10 minute was cooled to 860~900 ℃ of sintering 120~360 minutes then, can obtain high magnetoconductivity low temperature sintered chip inductive material.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1326805C (en) * | 2004-03-11 | 2007-07-18 | 横店集团东磁有限公司 | Low-temperature sintered NiCuZn ferrite material and its preparation method |
CN100440390C (en) * | 2004-12-10 | 2008-12-03 | 胜美达集团株式会社 | Ni-zn series ferrite compound and antenna coil |
CN116354713A (en) * | 2023-04-06 | 2023-06-30 | 电子科技大学 | NiCuZn soft magnetic ferrite material and preparation method thereof |
-
2002
- 2002-11-05 CN CN 02146687 patent/CN1405800A/en active Pending
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1326805C (en) * | 2004-03-11 | 2007-07-18 | 横店集团东磁有限公司 | Low-temperature sintered NiCuZn ferrite material and its preparation method |
CN100440390C (en) * | 2004-12-10 | 2008-12-03 | 胜美达集团株式会社 | Ni-zn series ferrite compound and antenna coil |
CN116354713A (en) * | 2023-04-06 | 2023-06-30 | 电子科技大学 | NiCuZn soft magnetic ferrite material and preparation method thereof |
CN116354713B (en) * | 2023-04-06 | 2024-02-09 | 电子科技大学 | NiCuZn soft magnetic ferrite material and preparation method thereof |
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